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Showing papers on "Thin-layer chromatography published in 2021"


Journal ArticleDOI
Yuangui Yang1, Zhengcai Ju1, Yingbo Yang1, Yanhai Zhang1, Li Yang1, Zhengtao Wang1 
TL;DR: In this review, a total of 219 articles published from 1980 to 2018 are investigated and it is expected that the review can provide a fundamental for further studies.

43 citations


Journal ArticleDOI
TL;DR: In this paper, the extraction of useful hydrocarbons (HCs) from used engine oil through solvent extraction followed by separation in a column via adsorption is reported, which could be extended to other useful compounds from used oils and concomitantly alleviating the related environmental pollution on larger scale.
Abstract: Engine oils are contaminated with hazardous species resulted from the oxidative degradation, which cause serious environmental issues. In this study, the extraction of useful hydrocarbons (HCs) from used engine oil through solvent extraction followed by separation in a column via adsorption is reported. n-Hexane, toluene, ethyl acetate, and their mixture (ethyl acetate/n-hexane) were used as solvent for extraction over powdered silica packed column, and the extracted samples were analyzed through thin layer chromatography, gas chromatography–mass spectrometry and Fourier transform infra-red spectroscopic techniques. Useful HCs like 1-fluoro heptane, n-hexane, methyl cyclopentane, toluene, p-xylene, o-xylene, toluene, benzaldehyde, 2,3-dimethyl pentane, and benzene-1,2-dicarboxylic acid were identified and subsequently distilled with respective percent recovery of 91, 71, 46, 45, 18, 08, 07, 06, 04 and 02%. The reported HC derivatives were obtained by interacting the sample oil with non-polar solvents (n-hexane and toluene) and slightly polar solvent (10% ethyl acetate/n-hexane mixture) in column which extracted the compounds having similar chemical nature in an appreciable amount via Londer dispersion forces and dipole-dipole interactions. The findings of this study concluded that the extraction of valuable benzene derivatives through highly cost-effective solvent extraction strategy is a promising alternative to the conventional burning and reclamation of spent engine oil. Witnessing the high efficiency and cost-effectiveness of the current process, it could be extended to the extraction of other useful compounds from used oils and concomitantly alleviating the related environmental pollution on larger scale.

19 citations


DOI
30 Sep 2021
TL;DR: In this article, the powder aerial parts of Haplophyllum tuberculatum were extracted with methanol and the extract was successively fractionated with different polarities of solvents.
Abstract: The aerial parts of Haplophyllum tuberculatum (H. tuberculatum) have traditionally been used by local communities to treat fever, gastrointestinal disorders, worms, malaria and fractures, however, the responsible ingredients of the selected medicinal plant have not been identified. In the present study, antibacterial and antioxidant ingredients were isolated and characterized from the plant parts of locally grown H. tuberculatum, and their biological activity was evaluated. The powder aerial parts were extracted with methanol and the extract was successively fractionated with different polarities of solvents. All polarities of extracts (hexane, chloroform, ethyl acetate, butanol, methanol and water) were used to determine their antibacterial and antioxidant activity by established in-vitro method. The disk diffusion and free radical scavenging 2,2-diphenyl-1-picrylhydrazyl (DPPH) methods were used to evaluate antibacterial and antioxidant activities of the prepared extracts and pure isolated compounds at different concentrations against three strains of Gram-positive and three Gram-negative bacteria. The antibacterial activity results showed that all prepared fractions and isolated pure compounds of the plant species gave significant activity against all Gram (+ and –) bacterial strains with the range of inhibition 0–20 mm. The antioxidant activity of the prepared extracts at all concentrations also showed substantial activity. Based on the highest activity, ethyl acetate and chloroform extracts were selected for the separation and isolation of antioxidant and antibacterial compounds by thin layer chromatography (TLC), column chromatography (CC), and preparative thin layer chromatography (PTLIC). The structure of the isolated antioxidant and antibacterial compounds from the ethyl acetate and chloroform extracts were determined on the basis of nuclear magnetic resonance (NMR) and mass spectra. The isolated pure compounds and active extracts could be used as a medicine for various infectious related diseases.

10 citations


Journal ArticleDOI
27 Feb 2021
TL;DR: In this article, the secondary metabolite profile from the fermentation of S. hygroscopicus was identified by Thin-Layer Chromatography (TLC) using a combination of solvents.
Abstract: Streptomyces hygroscopicus (S.hygroscopicus) is a Gram-positive soil bacterium that can produce secondary metabolites from fermentation that have a therapeutic effect. The fermented S. hygrocospicus metabolites that are still in the form of crude extracts are difficult to develop as drug preparations because the active compounds are not yet known, so it will be challenging to determine the dosage of drugs that have a therapeutic effect. Therefore, it is necessary to carry out exploratory research to narrow down the secondary metabolite profile from the fermentation of S. hygroscopicus, using extraction and fractionation methods, which are then identified by Thin-Layer Chromatography (TLC) using a combination of solvents. This study used the extraction method with a separating funnel. The fractionation was carried out using the BUCHI (Sepacore®) Flash Chromatography and Reveleris® PREP Purification System column chromatography gradually using ethyl acetate and n-hexana. 47 and 60 of the fractionation results were taken as samples, that further were profiled using TLC and given the appearance of 10% KOH stains and p-Anisaldehyde - sulfuric acid, so that various classes of compounds with different Rf values were obtained, namely Monoterpenes, Triterpenes, Steroids, Saponins, Coumarin, Scopoletin, and Alkaloids.

7 citations


Journal ArticleDOI
TL;DR: The combination of polar (acetone) and non-polar solvents (hexane) and the use of silica as stationary phase was efficient to recover and purify torularhodin from the intracellular pigments of Sporobolomyces ruberrimus.
Abstract: This work aimed at evaluating the influence of organic solvents and stationary phases in the extraction with glass beads and chromatographic purification of carotenoids, especially torularhodin, from Sporobolomyces ruberrimus. The combinations of acetone:hexane (1:1 v/v) and acetone:ethyl ether (1:1 v/v) yielded 171.74 and 172.19 μg of total carotenoids.g of cells-1, respectively. The first blend resulted in the highest percent of cell lysis of 57.4%. Among different proportions of acetone:hexane, the 9:1 v/v mixture showed a significant difference (p < 0.05), resulting in a recovery of total carotenoids of 221.88 μg.g of cells−1. The purification of carotenoids was made by preparative chromatography and the yield of the silica-containing stationary phase was higher (24 μg torularhodin.g cells−1). The analyses of the purified fractions in thin layer chromatography and high performance liquid chromatography indicated that the purification of carotenoids, especially of torularhodin, was successfully performed. The combination of polar (acetone) and non-polar solvents (hexane) and the use of silica as stationary phase was efficient to recover and purify torularhodin from the intracellular pigments of Sporobolomyces ruberrimus.

6 citations


Journal ArticleDOI
TL;DR: In this paper, the quantity and quality of phospholipid (PL) in edible insects (crickets, migratory locusts, and silkworms) were investigated using thin-layer chromatography (TLC), gas chromatography, and enzymatic methods.

6 citations


Journal ArticleDOI
TL;DR: In this paper, a compound from the fruit peel of Lysia domesticum (Lansium domesticum) was identified as 2-ethyl,3-(1'-hydroxy-2'-menthene) propenal and demonstrated the strongest cytotoxicity against T-47D, WiDr and Hep G2 cell lines.
Abstract: Lansium domesticum (fam. Meliaceae) contains various compounds with various biological activities. Based on the previous research, extracts from several parts of the plant have biological activity. This study aimed to isolate a compound from the fruitpeel of L. domesticum and evaluate cytotoxic activity against T47D, WiDr and HepG2 cell lines. Powdered peels were macerated with ethyl acetate and the filtrate was evaporated to give EtOAc extract. Dried extract was triturated with n-hexane to give n-hexane soluble fraction (A) and insoluble fraction (B). The fraction B was separated using vacuum column chromatography (VLC) with mobile phase n-hexane: ethyl acetate and given 5 fractions. Fractions B3-B5 were combined and separated using VLC with n-hexane and ethyl acetate as mobile phase. This VLC separation gave 18 subractions, subfractions 6-9 with the similar TLC profile were combined. This subfraction was separated further using preparative thin layer chromatography to give compound 1. The Isolated compound (1) appeared as liquid. The chemical structure of 1 was identified acoording to spectroscopic data and comparison with literature. Cytotoxic bioassay was performed on T-47D, WiDr and Hep G2 cell lines in a series of concentrations at 50, 40, 30, 20, 10 and 5µg/mL, with Doxorubicine used as positive control. According to spectroscopic data, compound 1 was identified as 2-ethyl,3-(1’-hydroxy-2’-menthene) propenal, and demonstrate the strongest cytotoxicity against T-47D cell lines (IC50=39.18+1.54 µg/mL).

6 citations


Journal ArticleDOI
TL;DR: In this article, a High Performance Thin Layer Chromatography (HPTLC) method for the determination of doxycycline hyclate was developed and validated using densitometry detection at 360 nm.
Abstract: According to World Health Organization (WHO) 10% of the medicines in the Low and Middle Income Countries (LMICs) are of poor quality posing a major public health threat. One way to circumvent such problem is the development and deployment of rapid, economical and efficient analytical methods. Hence this research aims to develop a High-Performance Thin Layer Chromatography (HPTLC) method for the determination of doxycycline hyclate. A rapid and simple HPTLC method with densitometry detection at 360 nm to determine doxycycline hyclate in capsules and tablet formulations was developed and validated. HPTLC was performed on glass plates coated with C18 reverse phase silica gel 60 F254 and pretreated with 0.27 M ethylenediaminetetraaceticacid (EDTA) solution. The mobile phase was dichloromethane: methanol: acetonitrile: 1% aqueous ammonia in the ratio of 10:22:53:15 (v/v). The linearity range lies between 200 and 1,000 ng/spot with correlation coefficient of 0.997. The Rf value is 0.5 ± 0.02%. Recoveries were in the range of 94.50–100.5%. Limit of detection and limit of quantitation values for doxycycline hyclate were 40 and 160 ng/spot respectively. The developed method was validated as per ICH guidelines. Thus, it was found to be accurate, precise, specific and robust. In forced degradation study, doxycycline hyclate was found to degrade in acidic and alkaline media, and through oxidative stress. The drug was found to be relatively stable to heat and photo degradation. The method was successfully applied for the routine quantitative analysis of dosage forms containing doxycycline hyclate. The developed method offered comparable results (as confirmed by F-test) with that of the HPLC pharmacopoeial (BP) analysis method.

5 citations


Journal ArticleDOI
TL;DR: A characteristic chemical fingerprint with clearly distinguishable features was established for T. sericea root bark that can be used for species authentication, and to select samples with high concentrations of a particular marker compound(s).
Abstract: Terminalia sericea is used throughout Africa for the treatment of a variety of conditions and has been identified as a potential commercial plant. The study was aimed at establishing a high-performance thin layer chromatography (HPTLC) chemical fingerprint for T. sericea root bark as a reference for quality control and exploring chemical variation within the species using HPTLC metabo3lomics. Forty-two root bark samples were collected from ten populations in South Africa and extracted with dichloromethane: methanol (1:1). An HPTLC method was optimized to resolve the major compounds from other sample components. Dichloromethane: ethyl acetate: methanol: formic acid (90:10:30:1) was used as the developing solvent and the plates were visualized using 10% sulfuric acid in methanol as derivatizing agent. The concentrations of three major bioactive compounds, sericic acid, sericoside and resveratrol-3-O-β-rutinoside, in the extracts were determined using a validated ultra-performance liquid chromatography-photodiode array (UPLC-PDA) detection method. The rTLC software (written in the R-programming language) was used to select the most informative retardation factor (Rf) ranges from the images of the analysed sample extracts. Further chemometric models, including principal component analysis (PCA) and hierarchical cluster analysis (HCA), were constructed using the web-based high throughput metabolomic software. The rTLC chemometric models were compared with the models previously obtained from ultra-performance liquid chromatography coupled with mass spectrometry (UPLC-MS). A characteristic fingerprint containing clear bands for the three bioactive compounds was established. All three bioactive compounds were present in all the samples, although their corresponding band intensities varied. The intensities correlated with the UPLC-PDA results, in that samples containing a high concentration of a particular compound, displayed a more intense band. Chemometric analysis using HCA revealed two chemotypes, and the subsequent construction of a loadings plot indicated that sericic acid and sericoside were responsible for the chemotypic variation; with sericoside concentrated in Chemotype 1, while sericic acid was more abundant in Chemotype 2. A characteristic chemical fingerprint with clearly distinguishable features was established for T. sericea root bark that can be used for species authentication, and to select samples with high concentrations of a particular marker compound(s). Different chemotypes, potentially differing in their therapeutic potency towards a particular target, could be distinguished. The models revealed the three analytes as biomarkers, corresponding to results reported for UPLC-MS profiling and thereby indicating that HPTLC is a suitable technique for the quality control of T. sericea root bark.

5 citations


Journal ArticleDOI
TL;DR: Two green, simple, and accurate chromatographic methods were developed and validated for the simultaneous determination of omeprazole and aspirin mixture in the presence of salicylic acid, a major impurity of aspirin.
Abstract: Two green, simple, and accurate chromatographic methods were developed and validated for the simultaneous determination of omeprazole and aspirin mixture in the presence of salicylic acid, a major impurity of aspirin. Method A is a reversed-phase ultra-high-performance liquid chromatography; the separation was performed on a C18 column, with a mobile phase composed of ethanol:0.1% aqueous solution of triethylamine acidified with orthophosphoric acid (pH 3) (30:70, v/v) at 0.15 mL/min flow rate and 230 nm. Omeprazole, aspirin, and aspirin impurity retention times were 7.47, 4.40, and 5.13 min, respectively. Good linearity was achieved in the concentration ranges of 5-80, 5-85, and 3-50 μg/mL for the three mentioned components, respectively. Method B is thin-layer chromatography (TLC) where silica gel TLC F254 plates were utilized to achieve separation using ethanol:ethyl acetate (2:8, v/v) as a developing system at 240 nm. The resulted Rf values were 0.83, 0.65, and 0.23 for omeprazole, aspirin, and impurity, respectively. The concentration ranges of 0.1-3 μg/band for the three drugs showed good linearity. The proposed methods are eco-friendly and greener when compared to the already reported method (Microchemical Journal, 152, 104350). This is the first use of TLC method for the determination of the three drugs. International Council for Harmonization (ICH) guidelines were followed to ensure the validity of developed methods.

5 citations


Journal ArticleDOI
01 Jan 2021
TL;DR: In this article, the synthesis of sophorolipids using waste syrup of Jaggery plant, non-edible Jaggery, oleic acid and corn oil was presented.
Abstract: Bio-surfactants are of importance due to their advantages in environmental compatibility, high biodegradability, low toxicity, high selectivity, specific activity, etc. compared to those of synthetic surfactants. Due to their eco-friendly character the demand for bio-surfactants is ascending. Bio-surfactants show applications in sectors such as medicine, personal care, paints, textile, pharmaceutics, etc. Sophorolipids (SLs) are effective surfactants and display promising applications as antimicrobial agents and in skin-healing properties. The present study involves synthesis of sophorolipids using waste syrup of Jaggery plant, non-edible Jaggery, oleic acid and corn oil. The synthesized sophorolipid was purified by solvent extraction & column chromatography. At an ,optimum combination of medium constituents, the yeast Starmerella bombicola (ATCC 22214) produced maximum yield of 42.9g/l of bio-surfactant at optimized pH control level. Sophorolipid was identified and purified by silica gel column chromatography and characterized using thin layer chromatography (TLC), Fourier-transform infrared spectroscopy (FTIR), high-performance liquid chromatography (HPLC), and liquid chromatography-mass spectroscopy (LC-MS). The surfactant properties of Sophorolipids such as surface tension, interfacial tension, foam stabilization, emulsification, and wetting were studied.

Journal ArticleDOI
TL;DR: An overview of bioautography procedure from extraction to structure elucidation of antimicrobial compounds from plants is given, showing planar chromatography in combination with biological detection can be an appropriate method of choice for fast, simple, and low-cost screening of plant extract for successful detection of antimacterial agents.
Abstract: Growing antibiotic resistance creates a need to find new antimicrobial agents characterized by diverse chemical structures and pharmaceutical activity. The higher plants synthesize many specialized...

Journal ArticleDOI
TL;DR: In this article, a study was carried out to investigate the metabolic profiling and free radical scavenging compounds in C. papaya fruit's pulp, peel and seeds through thin-layer chromatography-mass spectrometry (TLC-MS) bioautography.
Abstract: Objectives: Carica papaya Linn. a member of the Caricaceae family, is a tropical fruit, rich in various secondary metabolites owing to its antioxidant, anti-inflammatory, anti-diabetic, and antihelmintic properties. The study was carried out to investigate the metabolic profiling and free radical scavenging compounds in C. papaya fruit's pulp, peel and seeds through thin-layer chromatography-mass spectrometry (TLC-MS) bioautography. Methodology: Aqueous, hydroalcoholic and alcoholic extracts of fruit pulp and peel were prepared along with the hydroalcoholic and hexane extract of seeds. These were subjected to total phenol, flavonoid and free radical scavenging estimation. Qualitative and quantitative high-performance thin-layer chromatography analysis of the best extracts was performed followed by TLC-MS bio autography assay for the detection of free radical scavenging compounds. Results: C. papaya peel was noted to contain the highest phenol and flavonoid content, but the seeds showed better free radical scavenging activity. The hydroalcoholic extracts of pulp, peel, and seeds examined through TLC-bioautography showed the presence of chlorogenic acid, ellagic acid, quercetin, β-sitosterol, linoleic acid, and iso-oleic acid as potent free radical scavenging compounds. Liquid chromatography-mass spectrometry analysis showed the presence of β-carotene, lycopene, and β-cryptoxanthin in pulp and peel along with other carotenoids and benzyl isothiocyanate, linoleic acid, oleic acid, and methyl palmitate were the major compounds detected in seeds through gas chromatography-mass spectrometry analysis. Conclusion: This study has revealed that C. papaya fruit and seeds possess potent free radical scavenging compounds. Seeds which make up the waste material may be utilized in cosmetic industries as they signify rich antioxidants.

Journal ArticleDOI
TL;DR: In this paper, the authors evaluated the separation ability of AgNO3-silica gel TLC and showed high separation ability between THC isomers and among ∆9-THC, ∆8-THc, and CBD.
Abstract: Various forms of cannabidiol (CBD)-containing products are sold in Japan. CBD is easily converted to mixtures of ∆9-tetrahydrocannabinol (∆9-THC) and its isomer, ∆8-THC, using household chemicals like diluted hydrochloric acid. This ease of production increases concerns regarding production of homemade THC mixtures. It is difficult to separate ∆9-THC, ∆8-THC, and CBD using thin-layer chromatography (TLC) on conventional silica gel. The selectivity of TLC on silver nitrate-impregnated silica gel (AgNO3-silica gel) differs from that of conventional silica gel. This study thus aimed to evaluate the separation ability of AgNO3-silica gel TLC. To evaluate potential separation ability, standards of five THC isomers (∆9-THC, ∆8-THC, a pair of diastereomers of ∆10-THC, and ∆6a,10a-THC), CBD, CBN, and ∆9-THCA were analyzed by 10% AgNO3-silica gel TLC (developed using toluene, system A) and silica gel TLC [developed using n-hexane/diethyl ether (8:2, v/v), system B]. Then, mock homemade THC mixtures, prepared by heating crystalline CBD in acidic ethanol, were analyzed using systems A and B. System A showed clear separation between the five THC isomers and between ∆9-THC, ∆8-THC, CBD, and their by-products in the mock homemade THC mixture. However, system B did not separate some combinations of THC isomers and gave a single group-like spot to the THC mixture. AgNO3-silica gel TLC shows high separation ability between THC isomers and among ∆9-THC, ∆8-THC, and CBD. It will thus be useful for analyzing homemade THC mixtures.

Journal ArticleDOI
TL;DR: 131I-FA could be used as a tumor targeting agent for nuclear medicine applications and the fast reaction monitoring could be achieved using miniaturized chromatographic techniques.

Journal ArticleDOI
TL;DR: In this paper, a dichloromethanolic fraction of partitioned methanol root and shoot extract was analysed by silica gel column chromatography, thin layer chromatography and high-performance liquid chromatography combined with photodiode-array detector, and coupled to electrospray ionization with Q-Exactive Orbitrap mass spectrometry (HPLC-PDA-ESI-MSn) in positive ion mode.

Book ChapterDOI
TL;DR: The main constituents of the polar lipid fraction are glycerolipids and nonpolar lipids as mentioned in this paper, which are found in pteridophytes, bryophytes and algae.
Abstract: Lipid extracts from plants represent a mixture of polar membrane lipids and nonpolar lipids. The main constituents of the polar lipid fraction are glycerolipids, that is, galactolipids, sulfolipid, and phospholipids. In addition, betaine lipids are found in pteridophytes, bryophytes, and algae. Nonpolar lipids include the storage lipid triacylglycerol, wax esters, diacylglycerol and free fatty acids. The complex lipid mixtures from plant tissues can be separated by thin-layer chromatography (TLC) into different lipid classes. In most cases glass plates coated with a silica gel are used as stationary phase and an organic solvent as mobile phase. Different solvent systems are required to separate polar membrane lipids or nonpolar lipids by TLC. Depending on the complexity of the lipid mixture, lipids are separated using one- or two-dimensional TLC systems. Different dyes and reagents allow the visualization of all lipid classes, or the selective staining of glycolipids or phospholipids. Lipids can be isolated from the TLC plate for subsequent analysis, provided that nondestructive methods are used for visualization.

Journal ArticleDOI
TL;DR: In this paper, two stability-indicating chromatographic methods have been established and validated for concurrent determination of probenecid (PRO), colchicine (COL) along with the degradation product of COL deg.
Abstract: Two stability-indicating chromatographic methods have been established and validated for concurrent determination of probenecid (PRO), colchicine (COL) along with the degradation product of colchicine (COL deg). PRO and COL were exposed to a stress stability study, which includes acidic, alkaline, oxidative, photolytic and thermal degradations. Chromatographic methods included the use of thin layer chromatography (TLC-densitometry) and high performance liquid chromatography (HPLC). In the first method, separation was achieved by using aluminum TLC plates that were precoated with silica gel G.F254 as the stationary phase and ethyl acetate-methanol-33%ammonia (8:1:1, by volume) as a mobile phase. The obtained chromatograms were scanned at 254 nm. The second method was based on HPLC using a RP- C18 column with isocratic elution. Good separation was obtained through a mobile phase comprised of phosphate buffer pH 5-acetonitrile (70:30, v/v) at a flow rate of 1.0 mL min-1 and ultraviolet detection at 254 nm. Different parameters affecting efficiency of the two methods were studied accurately for optimum separation of the three cited components. The suggested methods were validated according to the International Conference on Harmonization (ICH) guidelines and were applied for bulk powder and commercial tablets.

Journal ArticleDOI
TL;DR: The capability of thin-layer chromatography-Gas Analyzer approach to analyze the isomers in this complex sample was demonstrated and showed good linearity of the calibration curves and acceptable recovery range.
Abstract: In this study, thin-layer chromatography was applied for selective extraction of volatile compounds in perfume prior to analysis with solid phase microextraction and gas chromatography-mass spectrometry. The standard compounds were desorbed from the thin-layer chromatography plate and extracted at 80°C for 15 min showing good linearity of the calibration curves (R2 > 0.98) and acceptable recovery range (65-81%). The plate after the separation was cut into four smaller parts followed by solid phase microextraction/gas chromatography-mass spectrometry analysis, which revealed different compound profile in each part with the correlation between log P of the standard compounds and their positions along the thin-layer chromatography plate (R2 = 0.65). This approach was applied to analyze perfume compounds in the sample with strong matrix interference from the synthetic agarwood. Terpene hydrocarbons (woody-based odors), ketones/esters, aldehydes, ethers, and alcohols were mostly observed at 8 ± 1, 6 ± 1, 5 ± 2, 4 ± 2, and 3 ± 2 cm, respectively, from the bottom of the thin-layer chromatography plate. While, the conventional solid phase microextraction/gas chromatography-mass spectrometry analysis of this sample solution revealed only 62 compounds (including 35 perfume compounds), the four-piece approach resulted in 109 compounds (62 perfume compounds). Furthermore, the capability of thin-layer chromatography-Gas Analyzer approach to analyze the isomers in this complex sample was demonstrated.

Proceedings ArticleDOI
16 Jan 2021
TL;DR: In this article, the authors used thin layer chromatography to determine the amount of MTP in a gout herbal sample and the results showed that the herbal gout powder samples were positive contains MTP.
Abstract: Based on data from the National Food and Drug Administration, there are 46 withdrawals of herbal products on the market because they contain hazardous chemicals such as MTP, phenylbutazone, dexamethasone, allopurinol, CTM, sildenafil citrate, tadalafil, and paracetamol. MTP is one of the analgesic-antipyretic drugs. However, MTP is widely known to be mixed into rheumatic herbs and gout. The use of high doses of MTP can cause side effects namely, stomach bleeding, palpitations, heart damage, and others. The purpose of this study was to determine the amount of MTP in a gout herbal sample. The sample used in this study was a sample of herbal gout powder sold in herbal stalls in the city of Tangerang. Samples are taken by random sampling method. The MTP qualitative analysis method uses thin layer chromatography. The stationary phase used was silica gel GF 254 while the mobile phase used consisted of methanol : ammonia (100: 1.5). The quantitative analysis method used the UV Spectrophotometry method with a maximum wavelength of 258.5 nm. Qualitative analysis showed that the Rf value of the herbal gout powder samples approached the Rf value of MTP and it was proven by the presence of purple spots under UV light. Furthermore, quantitative analysis showed that the levels of MTP contained in the herbal gout powder sample were 72.59±1.12 sample A, 65.34±1.13 sample B, 11.45±0.98 sample C, and 6.70±0.64 sample D, respectively. The results showed that the herbal gout powder samples were positive contains MTP.

Book ChapterDOI
TL;DR: In this paper, the authors outline protocols for the isolation, separation, and derivatization of plant lipids for subsequent gas chromatography and GC-MS analysis, including methods suitable for the analysis of lipid-bound or free fatty acids, long chain alcohols, and monoacylglycerols.
Abstract: Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) represent powerful tools for the quantitative and structural analysis of plant lipids. Here, we outline protocols for the isolation, separation, and derivatization of plant lipids for subsequent GC and GC-MS analysis. Plant lipids are extracted with organic solvents and separated according to their polarity by thin-layer chromatography or solid phase extraction. As most lipids are not volatile, the analytes are derivatized by transmethylation or trimethylsilylation to enable the transition of the molecules into the gas phase. After separation on the polymer matrix of the GC column, the analytes are detected by flame ionization or mass spectrometry. This chapter includes methods suitable for the analysis of lipid-bound or free fatty acids, long chain alcohols, and monoacylglycerols and for the determination of double bond positions in fatty acids.

Journal ArticleDOI
TL;DR: In this article, a crude extract of this isolate by Thin Layer chromatography (TLC) with the optimum solvent system (Methanol: Ethyl acetate, 40:60 v/v ratio) showed multiple bands at the retention factor values 0.9, 0.6 and 0.4 both under visible and UV light.
Abstract: Marine actinomycetes are potential sources of secondary metabolites with wide range of applications. In the current study, Streptomyces thermolineatus VITKV6A, which was screened from our previous study, was mass cultivated to obtain the active compound. Analysis of crude extract of this isolate by Thin Layer chromatography (TLC) with the optimum solvent system (Methanol: Ethyl acetate, 40:60 v/v ratio) showed multiple bands at the retention factor values 0.9, 0.6 and 0.4 both under visible and UV light. The individual compounds in the crude extract were eluted by silica gel column chromatography. The antimicrofouling activity of fraction 2 showed antimicrofouling activity against biofilm forming bacteria Psychrobacter celer VITKV3, Psychrobacter alimentarius VITKV4 and Kocuria rhizhophila with MIC of 0.5, 0.75 and 0 . 75 μ g /ml respectively. Similarly, the antimacrofouling activity of fraction 2 was examined by mollusc foot adherence assay against Patella sp. The percentage of fouling and regaining decreased with increasing concentration, whereas complete inhibition of fouling was observed at a concentration of 1000 μ g mL−1. The bioactive compound exhibited low cytotoxicity and higher LC50 value of 173 . 72 μ g mL − 1 against Artemia salina. HPLC analysis of the active fraction showed a single peak with retention time of 3.117 mins, which reveals the purity of the compound. Further, the active compound was characterized using gas chromatography coupled with mass spectroscopy (GC-MS), Fourier Transform Infrared Spectroscopy (FTIR) and NMR and identified as Oxycyclopentadien with alternative name 1,3-Cyclopentadien-1-ol. This compound is accountable for the antifouling properties of Streptomyces thermolineatus VITKV6A.

Journal ArticleDOI
16 Aug 2021
TL;DR: This study scientifically validates the traditional claim of M. charantia as an aphrodisiac or male fertility enhancer and suggests that 13, 14-epoxyoleanan-3-ol-acetate might be responsible for the observed activity.
Abstract: Introduction: Male infertility has been associated with oxidative stress induced and or microbial induced in some men. The use of medicinal plants to overcome oxidative stress induced infertility cannot be over emphasized. Hence, the aim of this research is to isolate antlipid peroxidation (an index of usage in treatment of oxidative stress induced male infertility) bioactive principle from Momordica charantia using bioactivity-guided isolation. Materials and Methods: n-Hexane fraction from crude ethanol extract obtained by Soxhlet extraction of aerial parts (without fruit) of bitter melon, M. charantia was assessed for in vitro lipid peroxidation, followed by bioactivity-guided isolation of bioactive principle using in vitro lipid peroxidation as index of aphrodisiac as well as male fertility enhancer. Results: Fractionation of active nhexane fraction using vacuum liquid chromatography (VLC) gave five pooled fractions on the basis of their TLC characteristics (nhexane: EtOAc, 2:3, sulphuric acid spray). In vitro activity of the most active VLC fraction C was less than that of positive control, vitamin E. Further fractionation of VLC-C by open column chromatography on silica gel led to isolation of a compound which was purified by preparative-TLC. The purified compound, 10 mg/mL (Rf 0.54, TLC Silica gel, nhexane: ethyl acetate; 2:3) was equipotent with vitamin E (25 mg/mL) in reducing peroxidation of polyunsaturated fatty acids in vitro. Structural elucidation by NMR (1H, 13C) and MS confirmed the identity of the new bioactive compound as 13, 14-epoxyoleanan-3-ol-acetate. Conclusion: This study scientifically validates traditional claim of M. charantia as an aphrodisiac or male fertility enhancer as well as suggest that 13, 14-epoxyoleanan-3-ol-acetate might be responsible for the observed activity.

Journal ArticleDOI
TL;DR: In this paper, stepwise pH gradient thin-layer chromatograms of biologically active substances with controlled developing solvent velocity are presented and described in the paper, and the reproducibility of the gradient retardation factor values of separated substance zones is satisfactory.

Journal ArticleDOI
TL;DR: In this article, the active principles present in Nux vomica with the toxicological action of the same were analyzed using High Performance Thin Layer Chromatography (HPTLC).
Abstract: Background: Chromatography is one of the important laboratory technique in which the components of a mixture are separated on an adsorbent in order to analyze, identify, purify and quantify a mixture. Thin Layer Chromatography (TLC)is used to support the identity of a compound in a mixture when the Rf of a compound is compared with the Rf of a known compound. High Performance Thin Layer Chromatography is a sophisticated and automated form of Thin Layer Chromatography (TLC). The procedure simultaneously processes the sample and standard that results in better analytical precision and accuracy at a faster pace. Pharmacological/ Toxicological action of Nux Vomica is because of its active principles present in the seeds namely strychnine, brucine etc. This research paper aims to corelate the active principles present in Nux Vomica with the toxicological action of the same. Materials and Methods: 1. Standard Nux Vomica mother tincture was tested for its alkaloid markers and its correlation with the toxicological action was studied. 2. Analysis of the mother tincture was done using High Performance Thin Layer Chromatography. 3. Stationary phase consisted of TLC Aluminium sheets with silica gel 60 F253 pre-coated layer (20cm x 10cm), thickness-0.2mm, no. of tracks-18, band length-6mm. 4. Mobile Phase consisted of Chloroform: Methanol (9.5:0.5). 5. The plate was developed in developing chamber and observed under U.V. Light. Results: Colours seen on the HPTLC Plates of samples are greenwhich corresponds to strychnine, dark blue which corresponds to brucine, orange to alkaloids fluorescent green to sterols and pink to fatty acids which are evident on the chromatogram. Conclusion: Therapeutic action of Nux Vomica as noted in Homoeopathic Materia Medica is because of the active principles like strychnine, brucine, alkaloids, sterols, fatty acids present in it which is evident from the chromatogram.

Journal ArticleDOI
TL;DR: In this article, a new chromatographic support was prepared from Local Syrian Clay (Bentonite), using thermal and acid treated Clay for utilizing it in thin layer chromatography (0.25mm thickness) to separate and determine of Paracetamol, Caffeine, and Aspirin in raw material and tablets.
Abstract: A new chromatographic support was prepared from Local Syrian Clay (Bentonite), using thermal and acid treated Clay (B500AW) for utilizing it in thin layer chromatography (0.25mm thickness) to separate and determine of Paracetamol, Caffeine, and Aspirin in raw material and in tablets. The separation carried out using mobile phase consisted of Cyclohexane-Chloroform- Methanol - acetic acid (14:5: 0.25:0.75) v/v. The specific surface area of treated bentonite was 45m2/g. Quantification was carried out densitometerically at λ = 250nm for Paracetamol, λ = 275nm for Caffeine, and at λ = 200 nm for Aspirin. The retardation factors (Rf) of Paracetamol, Caffeine, and Aspirin were 0.10, 0.21, and 0.40 respectively. Calibration curves were obtained in the concentration ranges of 5.0-40.0µg/spot, 2.0-16.0µg/spot and 3.0-24.0µg/spot for standard solutions of Paracetamol, Caffeine and Aspirin respectively. The New Prepared Chromatographic Thin Layers were successfully applied for analysis of commercial dosage forms (tablets) containing the drugs with average recovery 98.33 –101.83% with RSD not more than 3.86%.


Journal ArticleDOI
20 Aug 2021
TL;DR: In this paper, a method for monitoring transformations of heavy oil fractions during secondary processes of oil refining is proposed, which is based on the study of changes in the molecular weight characteristics by gel-permeation chromatography (GPC) using a refractometric detector.
Abstract: A rapid and easy to use method for monitoring transformations of heavy oil fractions during secondary processes of oil refining is proposed. The method is based on the study of changes in the molecular weight characteristics by gel-permeation chromatography (GPC) using a refractometric detector. Optimal conditions for registration of the chromatograms (temperature, eluent consumption and its composition) were specified. Heptane, toluene, and toluene added with 1% and 5% of methanol were studied as eluents, the polarity indices being arranged in a series 0.2; 2.4; 2.43; 2.54. The effect of the nature of the solvent on the type of the product chromatogram is determined. It is shown that addition of a polar solvent to a nonpolar one increases the polarity index, reduces both the degree of association of petroleum molecules and adsorption on the gel. The most available toluene which meets the GPC requirements is chosen as an eluent. Addition of 1% CH 3 OH to the eluent promotes suppression of polyelectrolyte effects and adsorption. The revealed absence of the dependence of the retained volume and the type of chromatograms on the eluent flow rate and temperature indicates that separation is carried out under conditions of exclusion and completely obeys the theory of exclusive liquid chromatography. The transformation of raw materials during a technological process of oil production at the JSC «ANKhK» was studied using the GPC method under above-mentioned chromatographic conditions. We have studied vacuum distillate of the primary oil refining unit ELOU+AVT-6 (VD) and the product of hydrocracking of the vacuum distillate of the 123PM unit (HVD). It is shown that determination of the molecular weight characteristics provides an important information about the behavior of technological processes. The HVD meets the requirements for hydrocracking products. A decrease in the content of aromatic hydrocarbons in comparison with the raw feedstock is proved by the data of thin layer chromatography (TLC).

Journal ArticleDOI
TL;DR: The dual retention mechanism in thin-layer chromatography taking place on three stationary phases of different polarity and using binary mobile phases composed of acetonitrile as the main component and water, or methanol as a modifier was confirmed.
Abstract: We investigated the dual retention mechanism in thin-layer chromatography taking place on three stationary phases of different polarity (C-18, plain silica gel and DIOL) and using binary mobile phases composed of acetonitrile as the main component and water, or methanol as a modifier. As the test analytes, we selected a set of 12 compounds of pharmaceutical importance and considerably different chemical structure, i.e. the imidazoline and serotonin receptor ligands, and their related compounds. Retention of each analyte in each investigated chromatographic system was determined in a wide enough range of the mobile phase composition, with volume fraction of the mobile phase modifier ranging from 0.10 to 0.90. Calculation of the exact turning point values as a proof of occurrence of the reversed-phase hydrophilic interaction chromatography (HILIC/RP) retention mechanism was based on the multimodal retention model. The dual retention mode was described with the use of the volume fraction of the mobile phase modifier, the total polarity and the total solubility models. For the DIOL, C-18 and silica gel stationary phase, the dual (HILIC/RP) retention mechanism was confirmed. In the case of the DIOL stationary phase and acetonitrile/methanol mobile phase, the observed retention mechanism was more complicated than the dual HILIC/RP one.

Journal ArticleDOI
TL;DR: In this article, the chemical composition of the steroids, triterpenoids and fatty acid methyl esters (FAMEs) in leaves of Carica papaya, which were analyzed by gas chromatography coupled with mass spectroscopy (GC-MS).
Abstract: Aim To extract and identify the non-polar entities from the leaves of Carica papaya, a plant used for medicinal purpose as folk medicine. Materials and methods Petroleum ether extract of the Carica papaya leaves was used for this study. Saponification process and methylation process was performed to separate fatty acids and unsaponifiable matters. Phytochemical constituents were separated using chemical process and separated fractions were analyzed by thin layer chromatography (TLC) and gas chromatography coupled with mass spectroscopy (GC-MS). Results The chemical composition of the steroids, triterpenoids and fatty acid methyl esters (FAMEs) in leaves of Carica papaya, which were analyzed by gas chromatography coupled with mass spectroscopy (GC-MS). A total of 15 fatty acid components were identified in saponifiable matter, from unsaponifiable portion 2 steroids (campesterol, β- or γ-sitosterol), 1 triterpene (squalene), and 1 diterpene (phytol) were identified. Conclusions The results indicate that the extract is rich in non-polar compounds. In this study, GC-MS method is at the central focus for identification of these phytoconstituents. The current method can be used for direct analysis of non-polar entities of plant material.